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Volume 28, Issue 10
Displaying 1-16 of 16 articles from this issue
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Research of deactivation methods for diatomaceous earth. IIYuzi TAKAYAMA1979 Volume 28 Issue 10 Pages 579-583
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn the previous report {Part I, Bunseki Kagaku, 20, 307 (1979)} a new silylation technique of Celite, diatomaceous earth, was developed by using hexamethyldisilazane (HMDS) vapor. However the deactivated Celite of a first class quality could not be obtained. In this report, a pretreatment method with HCl for deactivation of Celite was examined. Siloxane groups in Celite hydrolyze with HCl-treatment to yield silanol groups which react easily with silylating reagent. The more deactivated Celite could be prepared by silylating Celite pretreated with HCl by HMDS vapor. This HCl-pretreatment technique is as follows; Celite was dipped three times in diluted HCl (conc. HCl:H2O = 1 : 50) for 24h, in aqueous 1% NaOH solution for 1h, and then in diluted HCl (conc. HCl : H2O=1; 100), successively. After this treatment, Celite was silylated by the previous method. The deactivated Celite obtained by this method had a first class quality as a support for a column of gas chromatograph.View full abstractDownload PDF (1004K) -
Tamotsu OKUMURA, Tadayoshi NAGAOKA1979 Volume 28 Issue 10 Pages 584-587
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSReversed-phase thin-layer chromatographic separation of twelve kinds of benzodiazepine minor tranquilizers was studied by using two kinds of chemical bonding alkylsilyl silica gel (dimethylsilyl silica gel and octadecylsilyl silica gel) as stationary phase and three kinds of organic solvents (methanol, acetone and dioxane) containing water as mobile phase. The compounds tested were benzodiazepine, medazepam, chlordiazepoxide, estazolam, triazolam (3-H-1, 4-benzo-diazepine), chloxazolam, flurazepam, diazepam, chlordiazepam, nimetazepam, lorazepam and nitrazepam (1, 3-dihydro-2H-1, 4-benzodiazepine-2-one). When dimethylsilyl silica gel was used as stationary phase for the separation of these minor tranquilizers, methanol-water (2 : 1) was more effective than acetone and dioxane. Octadecylsilyl silica gel gave better separation than dimethylsilyl silica gel when the mobile phase (methanol-water=2:1 or 3:1) added with ammonium hydroxide was used. Thus, the reversed-phase thin-layer chromatography with chemical bonding alkylsilyl silica gels as stationary phase seems to have wide applications in the separation of various pharmaceuticals including benzodiazepine minor tranquilizers, cephalosporin antibiotics {T.Okumura : Bunseki Kagaku, 26, 848 (1977)} and steroidal hormones {T. Okumura, A. Azuma : Bunseki Kagaku, 28, 235 (1979)}.View full abstractDownload PDF (644K) -
Ikuei KIFUNE, Kikuo OIKAWA1979 Volume 28 Issue 10 Pages 587-590
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for the determination of trace amounts of ammonia and lower amines in the atmosphere was studied. Samples were collected at a flow rate of 6 l/min on a glass fiber filter (area of filter is 19.6 cm2) impregnated with a mixture of aqueous solutions of 8% oxalic acid and 1% glycerin. Ammonia and lower amines caught by this filter was extracted with water, and 1 ml of the extract was introduced into an ion chromatograph. Collection efficiencies of both ammonia and lower amines were nearly 100 % both in the above sampling conditions. Both ammonia and lower amines are recovered at almost 100 % efficiency, irrespective of the quantities added to the oxalic acid-glycerin. This technique was simple and collection and extraction efficiencies were good. The coefficient of variation of analysis was less than 5%. Samples collected were able to be kept for at least 6 days without any losses of ammonia and lower amines.View full abstractDownload PDF (761K) -
Tadao TAMURA, Kazutoshi TANABE, Jiro HIRAISHI, Shinnosuke SAËKI1979 Volume 28 Issue 10 Pages 591-595
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe moments of spectra are expected to be a good sifter for searching infrared spectra, as they represent the characteristics of spectral pattern. The efficiency of 1st, 2nd, 3rd, and 4th moments of infrared spectra has been examined. About 450 IRDC spectral charts have been digitized by use of a curve reader model JEOL JRS-80 for the frequency range from 4000 to 400 cm-1. The reproducibility of the reader is sufficient for the present purpose. Although the valueS of the moments depend on the experimental conditions, especially on the sampling technique for solid samples, it is concluded that the moments can be used as one of the sifters for searching infrared spectra. The efficiency is approximately 3% when the four moments are used, and 0.5% when the frequency of the strongest absorption band is used together with the four moments. Similar study has also been made for the frequency range from 2000 to 400 cm-1. The results indicate that the frequency range does not affect significantly the efficiency of the moments. As the result is more or less affected by the correction of the background of the observed spectra, it is desirable to measure the spectra under the normalized condition for improving the efficiency.View full abstractDownload PDF (754K) -
Takejiro TAKAMATSU, Munetsugu KAWASHIMA, Mutsuo KOYAMA1979 Volume 28 Issue 10 Pages 596-601
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAn ion chromatographic method for the determination of arsenite and arsenate ions in the extract of sediment was investigated. A Dionex Model 10 Ion Chromatograph (separator column: 3 mm φ × 500 mm, suppressor column : 6 mmφ × 250 mm) designed for anion analysis was used by connecting the concentrator column (3mmφ × 150 mm). The optimum eluent and flow rate for arsenate ion were 0.003 M NaHCO3-0.0014 M Na2CO3 and 137 ml/h, respectively. The procedure was as follows : A 500 mg dried sample was extracted with 5 ml of 1N HCl by shaking (30°C, 30 min). One ml aliquot of extract was taken and 5 ml of 5% triethanolamine was added. The solution was adjusted to pH 11.5 with NaOH and after the addition of (12) drops of hydrogen peroxide, diluted to 100 ml. Another 1 ml aliquot of extract was also adjusted to pH 11.5 and diluted to 100 ml after 20 ml of 10% crotonaldehyde-50% ethanol and 5 ml of 5% triethanolamine were added. Ten ml of each solution was injected into the system for analysis through the concentrator column. The concentrations of total arsenic and arsenate ion in the extract were determined in the range of 01 μg As without interference by diverse ions such as NO3-, PO43- and SO42-. By applying this method to the core sediment of Lake Biwa, it became apparent that all of the arsenic in the extract of the upper thin layer existed as arsenate ion but in a lower reduced layer {(14) cm from surface} the fraction arsenite ion increased to about 40%.View full abstractDownload PDF (1057K) -
Kunishige HIGASHI, Kazuyoshi HAGIWARA1979 Volume 28 Issue 10 Pages 601-606
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSTar balls sampled from the sea near Japan were characterized to make clear the present situation of oil pollution. A glass column (1.5 m × 3 mm i.d.) packed with 3% Silicone SE-30 on Chromosorb W was employed. Injection port temperature was 260 °C, and the column temperature was programmed from 80°C to 300°C at 10°C/min and held at 300°C. The carrier gas was nitrogen and the flame photometric detector was used to measure sulfur-containing compounds. Dehydrated oil sample was dissolved in benzene and 4μl of the solution was injected. Profiles of chromatograms were obtained for 8 crude oils (Minas, Murban, Iranian light, Iranian heavy, Kuwait, Hout, Oman and Khafji) imported to Japan. The sulfur content of Indonesian Minas crude oil was low, which was easily discriminated from the oils of the Middle East. Although the Middle East oils had similar profiles each other, the profile of Murban crude oil was the most characteristic of all. The discrimination was relatively easy among petroleum products such as lubricating oils and fuel oils A, B and C. The crude oils were weathered on a pool to study the effect of weathering of oil on a profile of chromatogram. The discrimination among the Middle East oils except Murban crude oil became difficult by the weathering. Chromatograms were measured on 15 samples of tar balls sampled in 1970 and 1973, and compared with those of the crude oils, the petroleum products, and the weathered oils. Nine samples were inferred to be formed from Minas-type crude oil, while four samples had similar profiles with those of the Middle East crude oils. Other two samples had uniqe profiles, which made it difficult to specify.View full abstractDownload PDF (753K) -
Naobumi OI, Masao HORIBA, Hajimu KITAHARA1979 Volume 28 Issue 10 Pages 607-610
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe gas chromatographic separation of enantiomers of various α-alkylphenylacetic acids {α-methylphenylacetic acid (I), α-ethylphenylacetic acid (II), α-isopro-pylphenylacetic acid (III), α-isopropyl-4-methylphenylacetic acid(IV), α-isopropyl-4-tert-butylphenylacetic acid (V), α-isopropyl-4-chlorophenylacetic acid (VI), α-isopropyl-4-methoxyphenylacetic acid (VII) and α-isopropyl-4-bromophenylace tic acid (VIII)} in the form of isopropylamide and tert- butylamide with an optically active stationary phase has been studied. These α-alkylphenylacetic acid alkylamides were resolved into their antipodes with separation factors ranging from 1.027 to 1.047 on a 40 m glass capillary column coated with N, N'-[2, 4-(6-ethoxy-1, 3, 5-triazine) diyl] bis (L-valyl-L-valyl-L-valine isopropyl ester). Rather high column temperature serves for the rapid elution. For example, the racemic α-methylphenylacetic acid isopropylamide has been separated within 15 min at 180°C. The separation factor for (VI), which is important compound as the acid moiety of a useful synthetic insecticide "SUMICIDIN®", is not so large, but it is sufficient for the determination of the optical purity that its resolution value is 1.84. It is noticed that the order of emergence observed on this phase is (+)-isomer before (-)-isomer in these carboxylic acids consistently. From the point of view of the absolute configuration it is concluded that the S-isomer emerges earlier than the R-isomer in every carboxylic acid with the exception of (V) of which absolute configuration is not yet determined, since the (+)-isomers of (I), (II), (III), (IV), (VI), (VII) and (VIII) are known to have the S-configuration. According to such regularity, it can be easily deduced that the (+)-isomer of (V) has also the S-configuration. We consider that this fact gives the interesting information on the diastereomeric intermolecular interactions of α-alkylphenylacetic acid enantiomers.View full abstractDownload PDF (743K) -
Yoshihito SUZUKI, Kazue TANI1979 Volume 28 Issue 10 Pages 610-615
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe ultraviolet (UV) detector has been the most widely used detector available for the determination of samples. While most aliphatic compounds exhibit little or no useful absorption in the UV region, they could be converted to the UV-absorbing derivatives. In this paper, high speed liquid chromatographic analysis of the trityl ether of aliphatic alcohols have been described. The derivatization of C1C14 aliphatic alcohols were accomplished with trityl chloride in pyridine solution at 80°C, for 30 min. Their derivatives were completly separated on a RP-18 column (4 mm i.d., 15 cm length) by methanol-water or methanol-2, 2, 4-trimethylpentane as a eluting solvent.View full abstractDownload PDF (757K) -
Masahisa FUJINAMI, Kozo NAGASHIMA, Yoshinori SUGITANI1979 Volume 28 Issue 10 Pages 616-618
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA rapid and simple fluorimetric method for the quantitative analysis of trace amounts of uranium was established. The procedure is as follows: A sample solution of about 500 ml containing less than 0.1 mg of uranium is acidified with (310) ml of concentrated hydrochloric acid, and is boiled for a few minutes to expel CO2 gas. To this solution are added each 50 ml portions of 4.6 × 10-2 M zinc nitrate and 3.6 ×10-2 M ammonium dihydrogenphosphate solutions, and pH is brought to 910 with aqueous ammonia. The UO22+ is then coprecipitated with Zn3(PO4)2. The fluorescence intensity of the uranyl ion by 365 nm excitation is measured at 520 nm. Quencher ions such as Mn2+ or large amounts of Ca2+ and Mg2+ cause the interferences. The separation of these ions is necessary prior to the application of the above procedure. The calibration curve was linear over the range of (0.0020.1) mg of uranium. This method was applied to the determination of uranium in the sea water at Oarai, with the result of 0.004 mg/l.View full abstractDownload PDF (354K) -
Hiroshi ONISHI, Yasuto KASHIWAGI1979 Volume 28 Issue 10 Pages 619-621
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn the precipitation of trace heavy metals as hydroxides, iron(III) hydroxide is usually used as collector. However, information on the precipitation of microgram amounts of iron as hydroxide is so scanty that this work was undertaken. Ten to 100μg of iron(III) could be precipitated almost quantitatively with 5.0 mg of aluminum(III) from 100 ml of sample solutions in the range of pH 6.5 to 8.5. The iron was determined photometrically with 1, 10-phenan throline. Diverse ions, such as fluoride, phosphate, tartrate, citrate and EDTA interfered with the precipitation of iron. However, the interference of 0.1 mmol of tartrate, citrate or EDTA could be eliminated by adding 1.0 g of ammonium peroxodisulfate to 100 ml of sample and boiling the solution for about 30 min at 0.05 M sulfuric acid.View full abstractDownload PDF (553K) -
Wataru YOSHIMURA1979 Volume 28 Issue 10 Pages 621-623
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSquare-wave polarographic determination of trace amounts of bismuth by separating coprecipitation with zirconium hydroxide was investigated. Thirty-two mg of zirconium oxychloride was added to a (501000) ml solution containing (0.633.15) μg of bismuth, and pH of the solution was adjusted to 9.7 with ammonia-water (1 : 1). The precipitate was separated by filtration and then dissolved in 25 ml of 4 M hydrochloric acid. The solution was diluted to 50 ml with distilled water, and a portion of this solution was subjected to the square-wave polarographic determination. Bismuth was collected most effectively with zirconium hydroxide from the solution adjusted to pH 9.7 with ammonia-water (1:1). The polarographic peak height was in linear relation with the concentration of bismuth in the range of (0.633.15) μg. The coefficient of variation was 1.0%. Among the various foreign ions examined, copper, antimony, zinc and nickel interfered with the polarographic determination remarkably.View full abstractDownload PDF (504K) -
Tetsuro MURAKAMI, Minori KAMAYA, Junichi SHINOZAKI, Yasuro KANARI1979 Volume 28 Issue 10 Pages 623-627
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSChrome Azurol S (CAS) was found to be effective for increasing the sensitivity of the barium chloranilate method for sulfate ion. On the treatment of sulfate ion {(525)μg} with barium chloranilate (40 mg) in 80% 2-propanol aqueous medium (17 ml), free chloranilate anion was released stoichiometrically by the sulfate. The precipitate of barium sulfate was filtered off. The chloranilate in a portion (15 ml) of the filtrate was then separated from the 2-propanol on a column (10 cm, diam. 5 mm) of activated alumina (0.16 g), by washing the column with water and eluting the chloranilate with 4 ml of 0.1 M aqueous ammonia. The chloranilate anion in the eluate was extracted with tris (1, 10-phenanthroline)iron(II), Fe(phen)32+, at pH2 into nitrobenzene (5ml) as an ion-pair complex. After removal of the aqueous layer the nitrobenzene layer was shaken again with 12.5 ml of an aqueous solution (pH 5) containing CAS (10-5 M) for 3 min. The chloranilate in the complex was quantitatively replaced by CAS, thus forming CAS-Fe(phen)3 complex in the nitrobenzene. The absorbance of the CAS complex was measured at 600 nm with 1-cm cells against a reagent blank. The ε value of the present method was 2.3 × 104lmol-1cm-1. For a rain sample containing 2.20 ppm of sulfur oxides the coefficient of variation of 6.60% was obtained in six replicate determinations.View full abstractDownload PDF (934K) -
Hiroshi FUJINUMA, Kamihiko ITSUKI1979 Volume 28 Issue 10 Pages 627-629
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSince H. Bode has recommended the use of brucine as a substitute for stinking pyridine for the spectrophotometric determination of arsenic with silverdiethyldithiocarbamate (Ag-DDTC), this base has preferably used, despite of the low sensitivity. In this paper, the use of cinchonidine, as 0.1 % chloroform solution containing 0.25% Ag-DDTC, was proposed from our study on various organic bases, because of less odor and relatively high sensitivity. The apparent molar extinction coefficient of the colored species is 1.56×104 dm3 mol-1 cm-1 at 510 nm, which is higher than that with brucine and is somewhat lower than that with pyridine. The color developed is stable at least for an hour at room temperature. Amounts of arsenic up to 20 μg are determined by measuring the absorbance at 510 nm and by using a linear calibration curve with good reproducibility, the coefficient of variation being 2% at 10μg level. Cinchonine can also be used as an alternative base.View full abstractDownload PDF (515K) -
Yasuyuki HOSHIKA1979 Volume 28 Issue 10 Pages 629-632
Published: 1979
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA gas chromatographic identification of trace styrene in air was investigated using Tenax-GC precolumn (60/80 mesh, 16cm×4 mm i.d., glass), alkaline reaction precolumn (10% NaOH on Shimalite W, AW, 60/80 mesh, 8cm×4 mm i.d., glass plus Tenax-GC 60/80 mesh, 8cm×4 mm i.d., glass) and 2, 4-dinitrophenylhydrazine (2, 4-DNP) reaction precolumn (2% 2, 4-DNP on glass beads 30/60 mesh, 6 cm×5 mm i.d., glass plus Tenax-GC 60/80 mesh, 16 cm×4 mm i.d., glass). The peaks of styrene, isobutyl butyrate, hexyl formate, isobutyl methacrylate, methyl hexanoate, 2-heptanone and cyclohexanone overlapped, in the following analytical gas chromatographic conditions; stationary phase, SP-1200 +Bentone 34 (5%+1.75%) ; support, Chromosorb W, AW, DMCS 80/100 mesh; glass column, 3 m×3 mm i.d., glass; column temperature, 80°C; carrier gas (nitrogen) flow-rate, 50 ml/min. The peaks of esters have disappeared completely due to the formation of the corresponding alcohols and acids by using the alkaline reaction precolumn, whereas the peaks of carbonyl compounds have also disappeared completely using the 2, 4-DNP reaction precolumn, however the styrene passed through quantitatively these reaction precolumns.View full abstractDownload PDF (636K) -
Yoshimitsu HIRAO, Kiyoshi FUJII1979 Volume 28 Issue 10 Pages T43-T45
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSUsing successive quartz double distillation system FS-2 which was commercially supplied by Fujiwara Scientific Company, the highest purity of water was obtained in our laboratory routinely. Waters in first and second distillation chamber of this still were changed after 10 l distillation. Distillation rate was controlled to 5 l/d (DDW-1) and 10 l/d (DDW-2). Distillation system was settled in semi-clean lab (Lead concentration in the air was about 1 ng/m3) in Aoyama Gakuin University. DDW-1 and-2 were collected directly from still in 2 l polyethylene bottles and were shipped to C. Patterson's Laboratory of California Institute of Technology in U. S. A. for the determination of lead. Lead blanks of reagents and bottles were determined before analysis. The sample water was acidified to 0.1 N HNO3 and spiked with 30 ng of 208Pb and equilibrated for 3 h at 55°C. Lead was extracted with dithizone-chloroform solution, backextracted to 1 N HNO3 and dried in Teflon beaker. The lead isotope ratio was measured with a mass spectrometer in Caltech. The lead concentrations were 1.0 (DDW-1) and 0.7 (DDW-2) ng/kg. This water was pure enough for the ultra trace analysis for lead.View full abstractDownload PDF (480K) -
Yuetsu DANZAKI1979 Volume 28 Issue 10 Pages T46-T49
Published: 1979
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe determination of phosphorus in sintered materials of magnesium-phosphoric acid and of magnesium-phosphoric acid-lanthanide oxide were described. These materials contain iron and aluminum less than 0.1%. For materials containing no lanthanide, after sample had been dissolved in nitric acid, magnesium and phosphorus were simultaneously determined by a modified L. Szekeres' method {Microchem. J., 19, 330 (1974)}. For materials containing lanthanides, after the phosphate had been precipitated as bismuth phosphate by excess of bismuth nitrate, phosphorus was determined by titration of unconsumed bismuth with EDTA in the presence of Xylenol Orange indicator.View full abstractDownload PDF (663K)
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